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THE ANNALS OF UNIVERSITY “DUNĂREA DE JOS “ OF GALAŢI FASCICLE VIII, 2006 (XII), ISSN 1221-4590 TRIBOLOGY 73 ULTRASOUND ACTION ON STRENGTH PROPERTIES OF POLYCRYSTALLINE METALS Luminiţa MORARU Physics Department, Faculty of Sciences, University of Galati, Galati, Romania. [email protected] ABSTRACT The mechanical properties of pure aluminum were investigated by tensile test on the sample with average grain size between 60 and 1000 µm. The stress strain functions given by the models are fitted to the measured points. The grain size dependence on the uniform yield stress was studied. In order to put in evidence the effect of ultrasonic field on grain size, the measurements were carried out for samples solidified under similar conditions both with and without sonication. For pure aluminium, the author quantitatively evaluated the validity of Hall-Petch model. KEYWORDS: Yield stress, grain size, ultrasonic field, acoustic streaming, cavitation. 1. INTRODUCTION One of the underlying principles in materials science is that properties can be deduced from knowledge of the microstructure. By microstructure we mean the crystalline structure and all imperfections, including their size, shape, orientation, composition, spatial distribution etc. In the cast of polycrystalline metals the deformation process becomes more complicated even in pure metals because of the grain boundaries. The effect of the grain size on the strength properties of polycrystalline metals has been studied and the Hall-Petch (HP) equation describes the relationship between the yield stress σ and the grain size d as [2, 6-8]: σ = σ 0 + K y ⋅ d −1 2 (1) where σ0 and Ky are temperature dependence constants. The grain size dependence of the stress parameters characterizing the tensile tests was determinate. During solidification of the metals the most common growth morphology is the dendritic formation. In most of the castings manufactured by different methods, the dendritic growth will occur. When the solidifying process takes place in presence of ultrasonic field, the equiaxed aluminum grains appeared. The average grain size of aluminum grain is smaller. The presence of ultrasonic field in molten is equivalent to mechanical stirring of the melted metal. The advantages of this method are fine microstructure, reduced micro porosity and cracking; primarily all the aluminum dendrites will be transformed to spheroids/ellipsoids grains. This technique produces “nondendritic rheocast structure”. The room temperature plastic deformation behaviour of different samples (samples solidified in presence and in absence of ultrasonic field) of aluminum has been studied. By ultrasonic treatments, a wide range of grain sizes varying from 60 to 1,000 µm was obtained in this study. The Hall–Petch behaviour of the samples showed distinctly linear regions, one in the fine grain size range ( 60 µ m〈 d 〈 160 µ m ) in the ultrasonic solidification conditions and the other in the coarse grain size range ( 170 µ m〈 d 〈 1000 µ m ) in natural solidification conditions. The Hall–Petch parameter Ky was significantly higher in the fine grain regime than coarse grain regime. Hardness measurements were also performed. 2. EXPERIMENTAL SETUP The measurements of the stress-strain curves were carried out on 99.97% purity aluminum of composition given in table 1. The tensile tests were carried out at room temperature. We used samples solidified in presence and in absence of ultrasonic field. The ultrasonic field was created with a magnetostrictive transducer and an ultrasound generator, to generate continuous longitudinal waves into the liquid sample. We preferred to introduce the ultrasound waves through the bottom of the crucible. In this arrangement, there is no barrier between the ultrasound source and the melted metal. The stepped stainless steel horn was used to transmit the ultrasound to the molten and it is completely resistant to ultrasonic erosion. Typical operating parameters were frequency of 20.338 kHz THE ANNALS OF UNIVERSITY “DUNĂREA DE JOS “ OF GALAŢI FASCICLE VIII, 2006 (XII), ISSN 1221-4590 TRIBOLOGY and the nominal input power of 600 W. The acoustic power dissipated by ultrasonic probe in 1000mldeionized water at ambient temperature and pressure as a function of electrical input power was determined by calorimetry. These data were used to allow selection of the appropriate input power to give constant transmitted power. After the completion of measurements, the ultrasonic horn was examined microscopically. No attack of the stainless steel by liquid metal samples was observed in either case, so there was no evidence of contamination of the liquid metal by alloying. are given in table 2. The ultrasonic field presence caused hardness increased unto 28%. 11.0 10.0 9.0 0.8 1.0 1.2 1.4 1.6 - 1/2 d 1.8 2.0 - 1/2 ( mm 2.2 2.4 ) Fig. 1. The yield stress as a function of grain size (without ultrasound). 3. RESULTS AND DISCUSSIONS 14.5 with us 14.0 σ ( MPa ) Figures 1 and 2 show the yield stress as a function of grain size for samples solidified under similar conditions both with and without sonication. A linear relationship between σ and d −1 2 can be established and it shows that HP equation is valid. The scatter of experimental values is high and it can be explained by the experimental difficulties in the determination of the yield stress in this very soft material. Substituting the constants obtained for the fitted straight line into eq. (1), we obtained: σ = 9.095 + 0.714 ⋅ d −1 2 without ultrasound, σ = 9.620 + 1.166 ⋅ d −1 2 with ultrasound. The slope of the Hall-Petch plots (Ky values) is higher for samples solidified in ultrasonic field presence. This higher value (see figures 1 and 2) it is expected to be to twinning. However, this remark will be followed up by further investigation. The samples solidified in presence and in absence of the ultrasonic field present a different grain size due to various solidification conditions. The samples solidified without ultrasounds presence present the grain size significantly larger (fig. 3). When the solidifying process takes place in presence of ultrasonic field, the equiaxed fine-grained aluminum appeared. The average size of aluminum grain is smaller. The grain size was measured on transversal sections with areas of 40 mm2 after mechanical and electrochemical polishing in optical microscope equipped with image analyzer. Investigations in our laboratory on aluminum revealed superior mechanical properties for samples solidified in ultrasonic field. The mechanical properties obtained for the aluminum 10.5 9.5 Table 1. Chemical composition of sample (ppm). Fe Si Cu Zn 60 60 30 30 The grain size of specimens was determined using the linear intercept method in conjunction with a logarithmic Gauss distribution. To make individual hardness measurements for aluminium, Brinell hardness tests are widely used. without us 11.5 σ ( MPa ) 74 13.5 13.0 12.5 12.0 2.5 3.0 3.5 - 1/2 d - 1/2 ( mm 4.0 ) Fig. 2. The yield stress as a function of grain size (with ultrasound). a) b) Fig. 3. Microstructure of 99.97%Al; (a) without ultrasound and (b) with ultrasound. THE ANNALS OF UNIVERSITY “DUNĂREA DE JOS “ OF GALAŢI FASCICLE VIII, 2006 (XII), ISSN 1221-4590 TRIBOLOGY Without ultrasound With ultrasound Table 2. Hardness test values (HB) 1 2 3 4 5 21.8 21.8 22.0 22.2 22.3 28.0 27.9 28.2 28.2 28.0 It is known that grain boundaries could act as barriers to dislocation motion, but we also viewed a grain boundary as a sort of "film". If the properties of the grain boundary were known then a more complete analysis of their strengthening effect could be made. Grain boundaries are simply planar defects between adjacent grains, each grain having different crystallographic orientations. Low angle grain boundaries occur when the miss-orientation of the lattices of adjacent grains is less than 15°. These boundaries can be modeled as an array of edge dislocations. The structure of high angle grain boundaries is more complex. The other characteristics of grain boundaries are that they tend to attract impurities. In a sense, this might be thought of as a film which can either strengthen or weaken a material. Grain boundary segregation of impurities, however, does not always embrittle a material [9]. Grain boundaries are lattice imperfections and as such increase the free energy of the material. There is a tendency to minimize the contribution from grain boundaries and this involves reducing the grain boundary area to grain volume ratio, something which happens as the grains grow larger. While other factors can cause grains to grow, this is essentially the process involved in normal grain growth (also called ideal grain growth). Non-ideal grain growth occurs when grain growth is inhibited by the presence of a second phase or is restricted by the edges of the specimen. Ultrasonic action, cold work, pressure, magnetic fields, etc. also cause grain growth to deviate from the ideal case. The effect of grain size on the hardness properties of polycrystalline metals consists in increasing of hardness for the sample with finegrained structure. It is suggested that this morphology of ingot solidified in ultrasonic filed results from increased growth rate and smaller crystallite size. So, reducing the grain size of a polycrystalline material is an effective way of increasing its strength [4]. Under ultrasonic conditions, the acoustic flow takes place in the liquid metal. It is clearly demonstrated that the acoustic flows are associated with the ultrasound absorption, whatever its nature. However, the absorption coefficient is quite small for the liquid metals, so the increase in the temperature of the melt caused by absorption process has been eliminated. In these conditions, the reason for this prominent change in solidification kinetic is assumed to be large-scale acoustic streaming. Its effect is a permanent stirring of the melt so the effects of thermal and mass homogeneity of the melt are quite obvious [3]. The increasing in the intensity of fluid 75 flow can give rise to grain multiplication, which can be attributed to the increased effective nucleation rate caused by the extremely uniform temperature and composition fields in the bulk liquid at early stages of solidification. Also, the forced convection increases the growth rate. The solidification starts by heterogeneous nucleation at the crucible wall through the so- called “big-bang” mechanism. Only a fraction of the nuclei formed at this stage contributed to the formation of the chilled zone and the majority of the nuclei are transferred into the hotter bulk liquid and remelted. The final solidified microstructure depends largely on the amount of nuclei surviving after the big-bang nucleation. Under the ultrasound action both the temperature and composition fields of the liquid metal are extremely uniform. The nuclei formed will survive due to the uniform temperature field, resulting in an increased effective nucleation rate. In addition, the intensive stirring may also disperse the cluster of potential nucleation agents, giving rise to an increased number of potential nucleation sites. Also, under forced convection, the nucleation and the growth at the chilled wall were suppressed, while the nucleation and growth in the bulk liquid were enhanced [1]. It has been suggested that the forced convector fluid flow induced by ultrasound may be sufficient to break small dendrite arms and distribute them throughout the melt. If a high energy boundary is formed in a metal in contact with its liquid then the condition indicates that the grain boundary will be wetted by the liquid phase, i.e. replaced by a thin layer of liquid and thus the dendrites break appear. Further these broken dendrites act as nucleants and grow as globular nondendrite structures. The acoustic streaming produced the change in possibility that hydrodynamic force to cause breakage of dendritic arms under the solidification conditions. In the same time, due to supplementary energy contribution, the ultrasonic field presence hinders the long-range ordering processes of atoms. At this moment, they act as nuclei for the growth of more particles and the relatively small dendrite spacing are created. The possibility that fluid flow could disrupt the crystal bonding is also considered [5]. The shear forces resulting from natural convection flow of the melt are too weak to disrupt the crystal bonding during solidification. However under ultrasonic field, these forces are dramatically increasing. The accuracy of sonic measurements is reasonable taking into account the difficulties associated with getting the ultrasound into the melted metal. The ultrasonic field presence into a liquid causes cavitation phenomenon [1]. This imposes a sinusoidal variation in pressure on a steady state ambient pressure. One new question of this study is the problem of cavitation and its microstreaming effect. The effect of ultrasound increases with increasing power, but not indefinitely since there is an optimum value beyond which the effect diminishes. 76 THE ANNALS OF UNIVERSITY “DUNĂREA DE JOS “ OF GALAŢI FASCICLE VIII, 2006 (XII), ISSN 1221-4590 TRIBOLOGY When 20.338 kHz high-intensity ultrasound was applied to the molten system, a mixing of the melted metal close to the solid-liquid interface and the crucible wall due to cavitation was produced. Near the solid surface, cumulative jets can be generated and the diffusion layer is thinned due to enhanced mass transport resulting from microstreaming. In our experiment, these optimum conditions in cavitation were studied in deionized water at ambient temperature. The ultrasonic treatment of liquid metals differed essentially from that of aqueous solutions and organic liquids. This is due to the different nature of cavitation nuclei and, hence different conditions required for the initiation and development of acoustic cavitation. Only fine solid particles (mainly oxides, e.g. Al2O3 in aluminum melt) can act as cavitation nuclei in metallic melts. At the same time, because the molten metals feature light opacity, the cavitation cannot be studied directly. 4. CONCLUSION In the cast of polycrystalline metals the deformation process has been studied related with the grain size in order to highlight the strength properties of polycrystalline metals and to study the applicability of the Hall-Petch (HP) equation. A linear relationship between σ and d −1 2 can be established and it shows that HP equation is valid. This study was making for samples solidified under similar conditions both with and without high power ultrasonic field presence. Our investigations on aluminum revealed superior mechanical properties for samples solidified in ultrasonic field. Studies into the Hall-Petch relationship show that the factor K is different in tension and compression. No systematic studies have been done on the effects of solutes on the K values and the difference in tension and compression. In future this represents another aims to investigate. REFERENCES 1. Abramov O.V., 1993, Ultrasound in liquid and solid metals, Russian Academy of Sciences, Moscow, (in English). 2. Kassner M.E., Li X., 1991, The Mechanical Properties of inSitu Composites, Scripta Metall. And Mater, vol. 25, pp. 28332860. 3. Moraru L. 2005, The effect of fluid flow on solidification of light metal alloy, Transaction of the University of Kosice, vol. 5, pp. 70-75. 4. Moraru L., 2003, Mechanical properties of 99,97% Al related to grain size and ultrasonic influence, U.P.B. Sci Bull., Seria B, vol. 1, No 65, pp. 59-65. 5. Moraru L., Tudose C., 2004, Analytic model of bonding forces in liquid metals and ultrasound influence, Proc. of 2nd Int. Conf. Romanian Acoustical Society, Impuls Publishing House, Bucureşti, pp. 75-80. 6. Petch N.J., 1953, The cleavage strength of polycrystals, J. Iron and Steel Inst., vol. 147, pp. 25-28. 7. Singh K.K., Sangal S., Murty G.S., 2002, Hall–Petch behaviour of 316L austenitic stainless steel at room temperature, Materials Science and Technolog,y , vol. 18 (2), pp. 165-172(8) 8. Singh K.K., 2004, Strain hardening behaviour of 316L austenitic stainless steel, Materials Science and Technolog,y , vol. 20 (9), pp. 1134-1142(9). 9. Song H.W., Guo S.R., Hu Z.Q., 1999, A coherent polycrystal model for the inverse Hall-Petch relation in nanocrystalline materials, Nanostructured Mater., vol. 11(2), pp. 203-210.